CN106045911A - Method for purifying pyraclostrobin by vapor deposition - Google Patents
Method for purifying pyraclostrobin by vapor deposition Download PDFInfo
- Publication number
- CN106045911A CN106045911A CN201610524961.1A CN201610524961A CN106045911A CN 106045911 A CN106045911 A CN 106045911A CN 201610524961 A CN201610524961 A CN 201610524961A CN 106045911 A CN106045911 A CN 106045911A
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- China
- Prior art keywords
- pyraclostrobin
- glass tubing
- glass tube
- white solid
- glass
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07D—HETEROCYCLIC COMPOUNDS
- C07D231/00—Heterocyclic compounds containing 1,2-diazole or hydrogenated 1,2-diazole rings
- C07D231/02—Heterocyclic compounds containing 1,2-diazole or hydrogenated 1,2-diazole rings not condensed with other rings
- C07D231/10—Heterocyclic compounds containing 1,2-diazole or hydrogenated 1,2-diazole rings not condensed with other rings having two or three double bonds between ring members or between ring members and non-ring members
- C07D231/14—Heterocyclic compounds containing 1,2-diazole or hydrogenated 1,2-diazole rings not condensed with other rings having two or three double bonds between ring members or between ring members and non-ring members with hetero atoms or with carbon atoms having three bonds to hetero atoms with at the most one bond to halogen, e.g. ester or nitrile radicals, directly attached to ring carbon atoms
- C07D231/18—One oxygen or sulfur atom
- C07D231/20—One oxygen atom attached in position 3 or 5
- C07D231/22—One oxygen atom attached in position 3 or 5 with aryl radicals attached to ring nitrogen atoms
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Pharmaceuticals Containing Other Organic And Inorganic Compounds (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
A method for purifying pyraclostrobin by vapor deposition includes steps: (1) respectively extracting crude pyraclostrobin with ammonium hydroxide and deionized water, performing vacuum distillation and desolvation, filtering, washing and drying to obtain a yellow oily substance; (2) transferring the yellow oily substance obtained at the step 1 into a glass tube, and sealing an opening of the glass tube by oxy-acetylene flame under protection of nitrogen; (3) heating the sealed glass tube in a drying oven for 1h at 230 DEG C to gasify the yellow organic substance; (4) taking out the glass tube, cooling to the room temperature, and collecting white solid; (5) dissolving the white solid obtained at the step 4, filtering, and performing vacuum rectification. According to the method for purifying pyraclostrobin by vapor deposition, high-boiling-point substances can be separated effectively, and a pyraclostrobin mixture obtained by separation is subjected to vacuum rectification to obtain pyraclostrobin with purity higher than 95%. The method is simple in operation and low in cost, and impurity separation can be well realized to achieve purification.
Description
Technical field
The present invention relates to the purification of product pyraclostrobin, be specifically related to a kind of vapour deposition process and purify pyraclostrobin
Process.
Background technology
Pyraclostrobin is the methoxy acrylic bactericide having pyrrazole structure concurrently, and 1993 public by Germany's BASF
Department finds, calendar year 2001 registers and lists, has been used at present in 100 various crop.2009, it is beautiful that its sales volume reaches 7.35 hundred million
Unit, is only second to Fluoxastrobin, becomes world's second largest antibacterial.Pyraclostrobin wide spectrum, efficiently, toxicity low, to non-target organism
Safety, to user and environment all safety close friends, is good market prospect in strobilurin series bactericidal agent, patent will mistake
The staple product of phase.
Owing to pyraclostrobin is in preparation process, use the materials such as a lot of organic solvent, various acid, alkali so that product
Yield and the purity of pyraclostrobin are greatly affected.Existing method of purification mainly use rectification, extract, the side such as filtration
Method, method technique is simple, cost is relatively low for these, but can not improve yield and the purity of pyraclostrobin, causes the wave of raw material
Take.
Summary of the invention
For the deficiencies in the prior art, the invention provides the technique side that a kind of vapour deposition process purifies pyraclostrobin
Method.
The present invention can be achieved through the following technical solutions:
A kind of vapour deposition process purifies the process of pyraclostrobin, it is characterised in that described method includes following step
Rapid:
(1) thick for pyraclostrobin product ammonia and the deionized water of 1 weight portion are extracted twice respectively, collect organic
Layer, decompression distillation is sloughed methylene chloride, is refiltered, washes, obtains yellow oily material after drying；
(2) the yellow oily material obtained in step 1 is transferred in glass tubing, under nitrogen protective effect, use oxy arc
By glass ferrule；
(3) glass tubing of good seal is put into and baking oven heats under conditions of 230 DEG C 1h so that yellow Organic substance gasifies；
(4) glass tubing taking-up being gradually cooling to room temperature, the different types of Organic substance after gasification is cold at glass tubing simultaneously
But can be deposited on positions different in glass tubing during, collect white solid；
(5) white solid in step 4 adds methylene chloride, stir 0.5h, carry out after insoluble matter is filtered
Rectification under vacuum, control rectification temperature, between 190-230 DEG C, is collected the fraction at a temperature of this, i.e. be can get high-purity pyrazoles ether
Bacterium ester.
The invention have the benefit that the different organic boiling points of employing are different, gasification degree is not at different temperature
Equally, being gasified at relatively high temperatures by pyraclostrobin, then cool down, i.e. can be deposited in glass tubing, this method can effectively be divided
From high boiling substance, then by the pyraclostrobin mixture of isolated by rectification under vacuum, i.e. can get purity be 95% with
On product pyraclostrobin.This method is the most simple to operate, low cost, moreover it is possible to well realize magazins' layout, reaches purification
Purpose.
Detailed description of the invention:
By embodiment, the detailed description of the invention of the present invention is made an explanation below.
Embodiment
A kind of vapour deposition process purifies the process of pyraclostrobin, and its process comprises the following steps: (1) will
The thick product of pyraclostrobin of 0.3 the weight portion ammonia of 1 weight portion and the deionized water of 1 weight portion are extracted twice respectively, receive
Collection organic layer, decompression distillation is sloughed methylene chloride, is refiltered, washes, obtains yellow oily material after drying；(2) will step
The yellow oily material obtained in rapid 1 is transferred in glass tubing, with oxy arc by glass ferrule under nitrogen protective effect；
(3) glass tubing of good seal is put into and baking oven heats under conditions of 230 DEG C 1h so that yellow Organic substance gasifies；(4) by glass
Pipe takes out and is gradually cooling to room temperature, and the different types of Organic substance after gasification can be deposited on glass in glass tubing cooling procedure simultaneously
Positions different in glass pipe, collects white solid；(5) white solid in step 4 adds methylene chloride, stirring
0.5h, carries out rectification under vacuum after being filtered by insoluble matter, control rectification temperature, at 200 DEG C, collects the fraction at a temperature of this,
To high-purity pyraclostrobin.
The present invention uses different organic boiling point different, and gasification degree is different at different temperature, by pyrazoles ether
Bacterium ester gasifies at relatively high temperatures, then cools down, and i.e. can be deposited in glass tubing, and this method can efficiently separate high boiling substance,
Again by the pyraclostrobin mixture of isolated by rectification under vacuum, i.e. can get the product pyrazoles ether that purity is more than 95%
Bacterium ester.This method is the most simple to operate, low cost, moreover it is possible to well realize magazins' layout, reaches the purpose purified.
Claims (1)
1. the process of a vapour deposition process purification pyraclostrobin, it is characterised in that said method comprising the steps of:
(1) thick for pyraclostrobin product ammonia and the deionized water of 1 weight portion are extracted twice respectively, collected organic layer, subtract
Methylene chloride is sloughed in pressure distillation, refilters, washes, obtains yellow oily material after drying；
(2) the yellow oily material obtained in step 1 is transferred in glass tubing, with oxy arc by glass under nitrogen protective effect
Glass ferrule；
(3) glass tubing of good seal is put into and baking oven heats under conditions of 230 DEG C 1h so that yellow Organic substance gasifies；
(4) glass tubing taking-up being gradually cooling to room temperature, the different types of Organic substance after gasification is cooled at glass tubing simultaneously
Cheng Zhonghui is deposited on positions different in glass tubing, collects white solid；
(5) white solid in step 4 adds methylene chloride, stir 0.5h, reduce pressure after insoluble matter is filtered
Rectification, control rectification temperature, between 190-230 DEG C, is collected the fraction at a temperature of this, i.e. be can get high-purity pyraclostrobin.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610524961.1A CN106045911B (en) | 2016-07-02 | 2016-07-02 | A kind of process of vapour deposition process purification pyraclostrobin |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610524961.1A CN106045911B (en) | 2016-07-02 | 2016-07-02 | A kind of process of vapour deposition process purification pyraclostrobin |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN106045911A true CN106045911A (en) | 2016-10-26 |
| CN106045911B CN106045911B (en) | 2018-03-02 |
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| CN201610524961.1A Active CN106045911B (en) | 2016-07-02 | 2016-07-02 | A kind of process of vapour deposition process purification pyraclostrobin |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106928144A (en) * | 2017-03-16 | 2017-07-07 | 上海晓明检测技术服务有限公司 | A kind of preparation method of high-purity pyraclostrobin standard items |
Family Cites Families (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| DE4423612A1 (en) * | 1994-07-06 | 1996-01-11 | Basf Ag | 2 - [(Dihydro) pyrazolyl-3'-oxymethylene] anilides, process for their preparation and their use |
| BR112012004562B1 (en) * | 2009-09-04 | 2021-02-17 | Basf Se | process for preparing 1-phenylpyrazoles and compound |
| CN103396364A (en) * | 2013-04-11 | 2013-11-20 | 南京理工大学 | N-alkyloxy-N-2-[1-(4-halogenated phenyl)-3-pyrazolyloxymethyl]phenylalkyl carbamate |
-
2016
- 2016-07-02 CN CN201610524961.1A patent/CN106045911B/en active Active
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106928144A (en) * | 2017-03-16 | 2017-07-07 | 上海晓明检测技术服务有限公司 | A kind of preparation method of high-purity pyraclostrobin standard items |
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| CN106045911B (en) | 2018-03-02 |
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